Method and Device for the Continuous Production of Polymers by Radical Polymerization

a technology of radical polymerization and polymerization method, which is applied in the direction of liquid-liquid reaction process, transportation and packaging, chemical/physical/physico-chemical process, etc., can solve the problem that special materials that are extremely expensive should be dispensed, and achieve the desired activity of polymerization, and reduce the effect of molar mass distribution

Active Publication Date: 2014-03-27
BASF AG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Benefits of technology

[0216]When monomer, initiator and regulator are mixed in one initial charge in order to supply them together to a reaction zone, the mixture is not storage-stable even at room temperature, and instead starts to react. Such a reaction mixture has to be transferred immediately to the reaction zone.
[0217]Alternatively, monomer and an initiator of appropriately high decomposition temperature can be stored together at ambient temperature for a certain time and the regulator can be mixed in only immediately before the start of the reaction. In contrast, initiator and regulator generally cannot be premixed, since they can form, for example, a redox pair under some circumstances and tend to premature decomposition (free-radical formation), which lowers the desired activity for the polymerization down to inactivity.
[0218]Advantageously, the process according to the invention allows performance of a continuous free-radical polymerization at comparatively very low temperatures.
[0219]The inventive mixing of the reactants in the cold state has the advantage over the prior art processes that the mixing and the start of the reaction are completely separated from one another. It is thus possible to combine the defined start of the reaction and the course of the reaction which is temperature-controlled, i.e. conducted isothermally, in accordance with the invention to give an advantageously narrower molar mass distribution.
[0220]In addition, the process according to the invention allows performance of a polymerization at comparatively low temperatures and with comparatively short residence times.
[0221]For better completion of reaction of the monomers, it has been found to be advantageous to meter in further initiator or to add a base and to (partly) neutralize the acid. The neutralization allows the reaction to be accelerated greatly.

Problems solved by technology

Extremely expensive specialty materials should especially be dispensed with.

Method used

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  • Method and Device for the Continuous Production of Polymers by Radical Polymerization
  • Method and Device for the Continuous Production of Polymers by Radical Polymerization
  • Method and Device for the Continuous Production of Polymers by Radical Polymerization

Examples

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process example 1

[0227]An aqueous acrylic acid solution (50% by weight) was mixed at room temperature homogeneously with an aqueous sodium persulfate solution (2% by weight) by means of a micromixer and then homogeneously with an aqueous solution of 2-mercapto-ethanol (10% by weight) by means of a second micromixer. The resulting reaction solution was pumped in each case through a preheated reaction capillary whose temperature was controlled in an oil bath with a constant flow rate, and the reaction capillaries had different temperatures, materials, diameters and lengths according to table 1 (all feeds by means of laboratory HPLC pumps, from Bischoff).

[0228]In example 4, in a departure therefrom, an aqueous 7% by weight sodium persulfate solution and an aqueous 50% by weight solution of 2-mercaptoethanol were used.

[0229]In example 5, in a departure therefrom, an aqeuous 3% by weight 2,2′-azobis[2-(2-imidazolin-2-yl)propane] dihydrochloride solution (obtainable, for example, under the VA044 name from...

process example 2

[0231]The aqueous solution of acrylic acid and 2-acrylamido-2-methylpropanesulfonic acid

[0232](35:15% by weight) was fed to a micromixer continuously and homogeneously with an aqueous sodium persulfate solution (4% by weight), mixed therein and then mixed homogeneously at room temperature with an aqueous solution of sodium hypophosphite (10% by weight) in a second micromixer. The resulting reaction solution was pumped continuously with a defined flow rate through a reaction capillary whose temperature was controlled in an oil bath, and the reaction capillaries had different temperatures, materials, diameters and lengths according to table 3.

TABLE 3FlowInitiatorRegulatorInternalØLengthrate[% by[% byTemperatureExampleMaterial[mm]1)[m]1)[g / h]wt.]2)wt.]2)*[° C.]1stainless1.6 + 3.010 + 107302580steel1.45712stainless1.6 + 3.010 + 108302580steel1.45711.1)x + y means: In the first capillary, the internal diameter was x mm or the length was x m and, in the directly connected second capillary...

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Abstract

The present invention relates to a method for the continuous production of a polymer by radical polymerization, wherein at least three materials are mixed with microstructures in one or more mixers and are then polymerized in at least one reaction zone.

Description

CROSS REFERENCE TO RELATED APPLICATIONS[0001]This application is a divisional of U.S. application Ser. No. 12 / 990,734, filed Nov. 2, 2010, the entire contents of which is hereby incorporated by reference in this application in its entirety. U.S. application Ser. No. 12 / 990,734 is a national stage application (under 35 U.S.C. §371) of PCT / EP2009 / 055296, filed Apr. 30, 2009, which claims benefit of European application 08155607.8, filed May 2, 2008, the entire contents of each of which are hereby incorporated by reference in this application in its entirety.BACKGROUND OF THE INVENTION[0002]The present invention relates to a process for continuously preparing a polymer by free-radical polymerization, in which at least three feedstocks are mixed in one or more mixers with microstructures and then polymerized in at least one reaction zone.[0003]WO 99 / 54362 describes a process for continuously preparing polymers, in which at least two reactants are conducted through and combined by a micr...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): B01F5/06B01J14/00C08F2/10
CPCB01F5/0602B01J14/00C08F2/10C08F2/00C08F2/01C08F220/06C08F2/38C08F20/06B01F25/40B01J19/00B01F25/42
Inventor MATTMANN, WOLFGANGLOTH, WOLFGANGURTEL, BOLETTEGUTLICH-HAUK, ELKEWEIDL, CHRISTIAN HUBERTDAIANDREAS
Owner BASF AG
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